WO2019065760A1 - Melt-blown nonwoven fabric and filter - Google Patents
Melt-blown nonwoven fabric and filter Download PDFInfo
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- WO2019065760A1 WO2019065760A1 PCT/JP2018/035740 JP2018035740W WO2019065760A1 WO 2019065760 A1 WO2019065760 A1 WO 2019065760A1 JP 2018035740 W JP2018035740 W JP 2018035740W WO 2019065760 A1 WO2019065760 A1 WO 2019065760A1
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- molecular weight
- propylene
- polymer
- fiber diameter
- nonwoven fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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- B01D39/163—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin sintered or bonded
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- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
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- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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Definitions
- the present invention relates to meltblown nonwovens and filters.
- a non-woven fabric (also referred to as a melt-blown non-woven fabric or a melt-blown non-woven fabric) produced by the melt-blowing method is superior in flexibility, uniformity and compactness because it can thin fibers constituting the non-woven fabric compared with general spunbonded non-woven fabrics. ing. For this reason, the meltblown non-woven fabric is laminated alone or with other non-woven fabric, etc., and filters such as liquid filters and air filters, sanitary materials, medical materials, agricultural coating materials, civil engineering materials, building materials, oil adsorbents, automobile materials , Electronic materials, separators, clothes, packaging materials, etc.
- the fiber which comprises a nonwoven fabric the fiber of thermoplastic resins, such as a polypropylene and polyethylene, is known.
- filters are used for the purpose of collecting particulates present in a liquid or gas and removing the particulates from the liquid or gas. It is known that the efficiency with which the fine particles of the filter are collected (hereinafter also referred to as “collection efficiency”) tends to be excellent when the average fiber diameter of the fibers of the non-woven fabric constituting the filter is small and the specific surface area is large. It is done. It is also known that the smaller the particle size of the fine particles, the lower the collection efficiency.
- non-woven fabric having a small average fiber diameter for example, a non-woven fabric obtained by molding a resin composition containing polyethylene and a polyethylene wax by a melt-blowing method has been proposed (see, for example, Patent Documents 1 and 2).
- non-woven fabric laminate in which a non-woven fabric obtained by molding a resin composition containing polyethylene and polyethylene wax by a melt-blowing method and a spunbonded non-woven fabric composed of composite fibers formed from polyester and ethylene polymer. (See, for example, Patent Document 3).
- the inventors of the present invention have found that the nonwoven fabrics described in Patent Document 1 and Patent Document 3 are inferior in collection efficiency because the average fiber diameter is not sufficiently small. Moreover, it turned out that the nonwoven fabric described in patent document 2 has a small specific surface area, and is inferior to collection efficiency. Moreover, the manufacturing method described in patent document 4 and patent document 5 uses a special apparatus, and it turned out that production speed is slower than the usual meltblown method. Therefore, in the present invention, it is an object of the present invention to provide a non-woven fabric which can be manufactured by the usual melt-blowing method and is excellent in collection efficiency, that is, a small average fiber diameter and a large specific surface area, and a filter using the non-woven fabric. .
- the means for solving the above-mentioned subject are as follows. ⁇ 1> In the discharge curve in gel permeation chromatography, it has at least one peak top at a molecular weight of 20,000 or more and at least one peak top at a position of molecular weight less than 20,000, and the intrinsic viscosity [ ⁇ ] is A meltblown non-woven fabric comprising a propylene-based polymer of 0.50 (dl / g) to 0.75 (dl / g).
- the propylene-based polymer includes at least a high molecular weight propylene-based polymer A having a weight average molecular weight of 20,000 or more and a low molecular weight propylene-based polymer B having a weight average molecular weight of less than 20,000.
- the meltblown nonwoven fabric as described in>.
- ⁇ 4> The meltblown nonwoven fabric according to ⁇ 2> or ⁇ 3>, wherein the content of the high molecular weight propylene polymer A is 60% by mass to 92% by mass with respect to the total mass of the propylene polymer.
- ⁇ 5> The meltblown nonwoven fabric according to any one of ⁇ 2> to ⁇ 4>, wherein a melt flow rate (MFR) of the high molecular weight propylene polymer A is 1000 g / 10 minutes to 2500 g / 10 minutes.
- MFR melt flow rate
- ⁇ 6> The meltblown nonwoven fabric according to any one of ⁇ 1> to ⁇ 5>, wherein the weight average molecular weight of the propylene-based polymer is 20,000 or more.
- meltblown nonwoven fabric according to any one of ⁇ 1> to ⁇ 6> which is composed of fibers having an average fiber diameter of less than 1.1 ⁇ m.
- ⁇ 8> a specific surface area of 2.0m 2 /g ⁇ 20.0m 2 / g ⁇ 1 > ⁇ meltblown nonwoven fabric according to any one of ⁇ 7>.
- ⁇ 11> A filter comprising the meltblown nonwoven fabric according to any one of ⁇ 1> to ⁇ 9>.
- ⁇ 12> The filter according to ⁇ 11>, which is a filter for liquid.
- non-woven fabric which can be manufactured by the usual melt-blowing method and is excellent in collection efficiency, that is, a small average fiber diameter and a large specific surface area, and a filter using the non-woven fabric.
- FIG. 7 is a discharge curve of gel permeation chromatography of the melt-blown nonwoven fabric obtained in Example 1.
- a numerical range indicated by using “to” indicates a range including numerical values described before and after “to” as the minimum value and the maximum value, respectively.
- the melt-blown non-woven fabric of the present disclosure has at least one peak top at a molecular weight of 20,000 or more and at least 1 at a molecular weight less than 20,000 in a discharge curve (hereinafter also referred to as "GPC chart") in gel permeation chromatography (GPC). And a propylene polymer having an intrinsic viscosity [ ⁇ ] of 0.50 (dl / g) to 0.75 (dl / g).
- the propylene-based polymer constituting the meltblown non-woven fabric of the present disclosure not only has at least one peak top at a molecular weight of 20,000 or more, but also has at least one peak top at a molecular weight less than 20,000,
- the viscosity [ ⁇ ⁇ ⁇ ] of 0.50 (dl / g) to 0.75 (dl / g) makes it possible to reduce the average fiber diameter and increase the specific surface area when a meltblown nonwoven fabric is produced. It becomes. Therefore, by constituting a meltblown nonwoven fabric with such a propylene-based polymer, the particle collection efficiency is improved. In addition, since it is not necessary to use a special device, the production speed is excellent.
- the meltblown nonwoven fabric of the present disclosure comprises a propylene-based polymer.
- a propylene-based polymer refers to a polymer having a propylene content of 50% by mass or more.
- the propylene-based polymer has at least one peak top at a molecular weight of 20,000 or more and at least one peak top at a molecular weight less than 20,000 in an emission curve in GPC.
- a peak top appearing at a position of a molecular weight of 20,000 or more in the discharge curve of GPC will be referred to as "polymer side peak top”
- a peak top appearing at a position of molecular weight less than 20,000 will be referred to as "low molecular side peak top”.
- the number of the polymer side peak tops and the number of low molecular side peak tops may be calculated by counting only the peak tops derived from the propylene-based polymer.
- At least one of the polymer-side peak tops is located at a molecular weight of 20,000 or more, preferably 30,000 or more, and more preferably 40,000 or more.
- at least one of the polymer side peak tops is located in the range of 20,000 to 80,000, preferably in the range of 30,000 to 70,000, and in the range of 40,000 to 65,000. It is more preferred to be located. Within the above range, the average fiber diameter tends to be small, which is preferable.
- At least one of the low molecular weight side peak tops is located at a molecular weight less than 20,000, preferably at 15,000 or less, more preferably at 14,000 or less, and 13,000 or less It is further preferred to be located.
- at least one of the low molecular weight side peak tops is located in the range of molecular weight 400 to less than 20,000, preferably in the range of 400 to 15,000, and in the range of 1000 to 14,000. It is more preferably located, more preferably in the range of 2000 to 13,000, and particularly preferably in the range of 6000 to 13,000.
- fiber breakage during spinning hardly occurs and the spinnability remains high, and the average fiber diameter tends to be reduced, which is preferable.
- the weight average molecular weight (Mw) of the propylene-based polymer is preferably 20,000 or more, more preferably 30,000 or more, and still more preferably 35,000 or more.
- the Mw of the propylene-based polymer is preferably 100,000 or less, more preferably 80,000 or less, and still more preferably 60,000 or less. If Mw is less than the above upper limit value, the average fiber diameter tends to be small, and it is preferable that Mw is more than the above lower limit value because breakage of fibers during spinning is less likely to occur and the spinnability is high.
- a discharge curve in gel permeation chromatography (GPC) of a propylene-based polymer refers to a discharge curve when measured by the GPC method under the following apparatus and conditions.
- the weight average molecular weight (Mw) of the propylene-based polymer refers to a weight average molecular weight in terms of polystyrene measured by gel permeation chromatography under the following apparatus and conditions.
- the result of GPC measurement before spinning can be adopted as the result of GPC measurement of the non-woven fabric.
- the intrinsic viscosity [ ⁇ ] of the propylene-based polymer is 0.50 (dl / g) to 0.75 (dl / g). If the intrinsic viscosity [ ⁇ ] is less than 0.50 (dl / g), spinning defects such as broken threads are likely to occur. When the intrinsic viscosity [ ⁇ ] exceeds 0.75 (dl / g), the average fiber diameter is large and the specific surface area is small, and the collection efficiency is poor.
- the intrinsic viscosity [ ⁇ ] of the propylene-based polymer is preferably 0.52 (dl / g) to 0.70 (dl / g) from the viewpoint of suppression of spinning defects and the viewpoint of average fiber diameter and specific surface area. More preferably, it is 0.55 (dl / g) to 0.60 (dl / g).
- the intrinsic viscosity [ ⁇ ] of the propylene-based polymer is a value measured at 135 ° C. using a decalin solvent. Specifically, it is determined as follows. About 20 mg of a propylene-based polymer is dissolved in 15 ml of decalin, and the specific viscosity sp sp is measured in an oil bath at 135 ° C. After diluting 5 ml of a decalin solvent to the decalin solution to dilute, the specific viscosity sp sp is measured in the same manner.
- the propylene-based polymer may be a homopolymer of propylene or a copolymer of propylene and an ⁇ -olefin.
- the amount of the ⁇ -olefin copolymerized with propylene is smaller than that of propylene, and may be used alone or in combination of two or more.
- the ⁇ -olefin to be copolymerized preferably has 2 or more carbon atoms, and more preferably 2, 4 to 8 carbon atoms.
- Specific examples of such ⁇ -olefins include ethylene, 1-butene, 1-pentene, 1-hexene, 1-octene, 4-methyl-1-pentene and the like.
- the propylene-based polymer preferably has a propylene content of 70% by mass or more, more preferably 80% by mass or more, still more preferably 90% by mass or more, and a propylene homopolymer Is particularly preferred.
- a propylene content of 70% by mass or more more preferably 80% by mass or more, still more preferably 90% by mass or more
- a propylene homopolymer Is particularly preferred When the content of propylene in the propylene-based polymer is within the above range, the compatibility is excellent when the high molecular weight polypropylene polymer A described later and the low molecular weight polypropylene polymer B described later are included, and the spinnability is excellent. And the average fiber diameter tends to be smaller, which is preferable.
- the melt flow rate (MFR: ASTM D-1238, 230 ° C., load 2160 g) is not particularly limited as long as the propylene polymer can be melt-spun, and is usually 600 g / 10 min to 2500 g / 10 min. And preferably in the range of 1200 g / 10 min to 1800 g / 10 min.
- the propylene-based polymer having a peak top at each position of a molecular weight of 20,000 or more and a molecular weight less than 20,000 in the discharge curve of GPC is at least one of high molecular weight propylene-based polymer A having Mw of 20,000 or more, and Mw is It may be prepared by including at least one low molecular weight propylene polymer B which is less than 20,000. That is, it may be a mixture of the high molecular weight propylene polymer A and the low molecular weight propylene polymer B (hereinafter, also referred to as a “propylene polymer mixture”).
- a propylene-based polymer having a peak top at each position of a molecular weight of 20,000 or more and a molecular weight of less than 20,000 in the discharge curve of GPC carries out multi-stage polymerization, and appropriately adjusts the type of catalyst compound, number of stages of multi-stage polymerization, etc. It may be prepared.
- the Mw of the high molecular weight propylene polymer A is 20,000 or more, preferably 30,000 or more, and more preferably 40,000 or more.
- the Mw of the high molecular weight propylene polymer A is preferably 80,000 or less, more preferably 70,000 or less, and still more preferably 65,000 or less. Within the above range, the average fiber diameter tends to be small, which is preferable.
- the Mw of the high molecular weight propylene polymer A is preferably 20,000 to 80,000, preferably 30,000 to 70,000, and more preferably 40,000 to 65,000.
- the high molecular weight propylene polymer A may be a homopolymer of propylene or a copolymer of propylene and an ⁇ -olefin. Examples of copolymerized ⁇ -olefins are as described above. From the viewpoint of high compatibility with the low molecular weight polypropylene polymer B, the high molecular weight propylene polymer A preferably has a propylene content of 70% by mass or more, and more preferably 80% by mass or more. It is more preferable that it is 90 mass% or more, and it is especially preferable that it is a propylene homopolymer. When the compatibility is excellent, the spinnability is improved, and the average fiber diameter tends to be smaller, which is preferable.
- the high molecular weight propylene polymer A may be used alone or in combination of two or more.
- Density of the high molecular weight propylene polymer A is not particularly limited, for example, be a 0.870g / cm 3 ⁇ 0.980g / cm 3, preferably 0.900g / cm 3 ⁇ 0. It is 980 g / cm 3 , more preferably 0.920 g / cm 3 to 0.975 g / cm 3 , still more preferably 0.940 g / cm 3 to 0.970 g / cm 3 .
- the density of the high molecular weight propylene polymer A is 0.870 g / cm 3 or more, the durability, heat resistance, strength and stability with time of the obtained meltblown nonwoven fabric tend to be further improved.
- the density of the high molecular weight propylene polymer A is 0.980 g / cm 3 or less, the heat sealability and the flexibility of the obtained meltblown nonwoven fabric tend to be further improved.
- the density of the propylene-based polymer is determined by heat-treating the strands obtained at the time of melt flow rate (MFR) measurement at a load of 2.16 kg at 190 ° C. for 1 hour at 120 ° C., room temperature It says the value obtained by measuring with a density gradient tube according to JIS K7112: 1999 after slow cooling to 25 ° C.
- MFR melt flow rate
- the melt flow rate (MFR) of the high molecular weight propylene polymer A is not particularly limited as long as it can be used in combination with the low molecular weight propylene polymer B described later to produce a meltblown nonwoven fabric.
- the MFR of the high molecular weight propylene polymer A is preferably 1000 g / 10 min to 2500 g / 10 min, more preferably 1200 g / 10 min to 2000 g from the viewpoint of fineness of fiber diameter, specific surface area, spinnability, etc. It is 10 minutes, more preferably 1300 g / 10 minutes to 1800 g / 10 minutes.
- MFR of a propylene-based polymer refers to a value obtained by measuring under a condition of a load of 2.16 kg and 190 ° C. in accordance with ASTM D1238.
- the content of the high molecular weight propylene polymer A based on the total mass of the propylene polymer is preferably 60 mass% to 92 mass%, more preferably 62 mass% to 90 mass%, and 70 mass%. It is further preferable that the content is ⁇ 88% by mass.
- the content of the high molecular weight propylene polymer A is in the above range, the average fiber diameter tends to be small and the specific surface area tends to be large. In addition, the balance of spinnability, fiber strength, collection efficiency of fine particles, and filtration flow rate tends to be excellent.
- the total mass of a propylene-type polymer means the mass of the sum total of the polymer whose content rate of propylene with respect to all the structural units is 50 mass% or more.
- the content of the high molecular weight propylene polymer A is less than 70% by mass, it is preferable to design the Mw of the high molecular weight propylene polymer A to be high.
- the content of the high molecular weight propylene polymer A exceeds 95% by mass, it is preferable to design the Mw of the high molecular weight propylene polymer A to be lower.
- the low molecular weight propylene polymer B may be a wax-like polymer because the Mw is less than 20,000 and the molecular weight is relatively low.
- the Mw of the low molecular weight propylene polymer B is preferably 15,000 or less, more preferably 14,000 or less, and still more preferably 13,000 or less.
- the Mw of the low molecular weight propylene polymer B is preferably 400 or more, more preferably 1000 or more, still more preferably 2000 or more, and particularly preferably 6000 or more. Within the above range, fiber breakage during spinning hardly occurs and the spinnability remains high, and the average fiber diameter tends to be reduced, which is preferable.
- the Mw of the low molecular weight propylene polymer B is preferably 400 or more and less than 20,000, preferably 400 to 15,000, and more preferably 1,000 to 14,000, and 2,000 to 1 It is more preferably 30,000, and particularly preferably 6000 to 13,000.
- the low molecular weight propylene polymer B may be a homopolymer of propylene or a copolymer of propylene and an ⁇ -olefin. Examples of copolymerized ⁇ -olefins are as described above. From the viewpoint of excellent compatibility with the high molecular weight polypropylene polymer A, the low molecular weight propylene polymer B preferably has a propylene content of 70% by mass or more, and more preferably 80% by mass or more. It is more preferable that it is 90 mass% or more, and it is especially preferable that it is a propylene homopolymer. When the compatibility is excellent, the spinnability tends to be high, and the average fiber diameter tends to be smaller.
- the low molecular weight propylene polymer B may be used alone or in combination of two or more.
- the softening point of the low molecular weight propylene polymer B is preferably more than 90 ° C., and more preferably 100 ° C. or more. When the softening point of the low molecular weight propylene polymer B exceeds 90 ° C., the heat resistance stability during heat treatment or use can be further improved, and as a result, the filter performance tends to be further improved.
- the upper limit of the softening point of the low molecular weight propylene polymer B is not particularly limited, and, for example, 145 ° C. may be mentioned.
- the softening point of a propylene-based polymer refers to a value obtained by measuring according to JIS K 2207: 2006.
- the density of the low molecular weight propylene polymer B is not particularly limited, for example, be a 0.890g / cm 3 ⁇ 0.980g / cm 3, preferably 0.910g / cm 3 ⁇ 0.980g / cm 3 deli, more preferably 0.920g / cm 3 ⁇ 0.980g / cm 3, more preferably from 0.940g / cm 3 ⁇ 0.980g / cm 3.
- the density of the low molecular weight propylene polymer B is in the above range, the kneadability of the low molecular weight propylene polymer B and the high molecular weight propylene polymer A is excellent, and the spinnability and stability over time are excellent. There is a tendency.
- the method of measuring the density of the propylene-based polymer is as described above.
- the content of the low molecular weight propylene polymer B with respect to the total mass of the propylene polymer is preferably 8 mass% to 40 mass%, more preferably 10 mass% to 38 mass%, and 12 mass%. It is more preferable that the content be 30% by mass.
- the content of the low molecular weight propylene polymer B is in the above range, the average fiber diameter tends to be small and the specific surface area tends to be large. In addition, the balance of spinnability, fiber strength, collection efficiency of fine particles, and filtration flow rate tends to be excellent.
- the total mass of a propylene-type polymer means the mass of the sum total of the polymer whose content rate of propylene with respect to all the structural units is 50 mass% or more.
- the Mw of the low molecular weight propylene polymer B is preferably 400 to 15,000, more preferably 1,000 to 13,000, and particularly preferably 1,000 to 8,000. is there.
- the Mw of the low molecular weight propylene polymer B is preferably 1,000 to 15,000, more preferably 3,000 to 15,000, and still more preferably 5,000 to 1. It is 50,000.
- the average fiber diameter of the fibers constituting the meltblown non-woven fabric is preferably less than 1.1 ⁇ m, more preferably 0.3 ⁇ m to 1.0 ⁇ m, and still more preferably 0.5 ⁇ m to 0.9 ⁇ m.
- the average fiber diameter of the meltblown non-woven fabric is an electron micrograph (magnification of 1000 times) of the meltblown non-woven fabric, 100 arbitrary non-woven fibers are selected, the diameter of the selected fibers is measured, and the average value is said.
- the meltblown non-woven fabric preferably has a ratio of peak fiber diameter to average fiber diameter (hereinafter also referred to as “peak fiber diameter ratio”) exceeds 0.5 when the fiber diameter distribution is measured.
- peak fiber diameter ratio exceeds 0.5, the fiber diameter distribution is narrowed, and the fiber diameter is made more uniform. Therefore, the generation of gaps caused by the non-uniform fiber diameter is suppressed, and the particle capture efficiency tends to be further improved.
- the peak fiber diameter ratio is more preferably 0.53 or more, further preferably 0.55 or more.
- the upper limit of the peak fiber diameter ratio is not particularly limited, and may be, for example, 0.95 or less, or 0.90 or less.
- the measuring method of the average fiber diameter and peak fiber diameter in fiber diameter distribution is demonstrated.
- (1) Measurement of average fiber diameter A meltblown non-woven fabric was photographed at a magnification of 5000 times using an electron microscope "S-3500N" manufactured by Hitachi, Ltd., and the fiber width (diameter: ⁇ m) was randomly 1000 points. Measure and calculate the average fiber diameter ( ⁇ m) by number average. In order to randomize the measurement points of the fibers in the meltblown non-woven fabric, a diagonal line is drawn from the upper left corner to the lower right corner of the photographed photograph, and the width (diameter) of the fibers at the intersection of the diagonal line and the fibers is measured. Take a picture and measure it until the measurement point reaches 1000 points.
- the value of the geometric average of the minimum value and the maximum value of the x axis in the divided section is taken as the peak fiber diameter (mode diameter).
- the specific surface area of melt blown nonwoven fabric is preferably 2.0m 2 /g ⁇ 20.0m 2 / g, more preferably 3.0m 2 /g ⁇ 15.0m 2 / g, 3.5m 2 It is more preferable that the range is / g to 10.0 m 2 / g.
- the specific surface area can be further increased by using the propylene-based polymer of the present disclosure.
- the specific surface area of the meltblown nonwoven fabric is a value determined in accordance with JIS Z8830: 2013.
- the meltblown non-woven fabric can have the average fiber diameter and the specific surface area in the above ranges by using the propylene-based polymer of the present disclosure, and is excellent in collection efficiency when it is used as a filter.
- the average pore diameter of the meltblown non-woven fabric is preferably 10.0 ⁇ m or less, more preferably 3.0 ⁇ m or less, and still more preferably 2.5 ⁇ m or less.
- the average pore diameter of the meltblown non-woven fabric is preferably 0.01 ⁇ m or more, more preferably 0.1 ⁇ m or more.
- the maximum pore diameter of the meltblown nonwoven fabric is preferably 20 ⁇ m or less, more preferably 6.0 ⁇ m or less, and still more preferably 5.0 ⁇ m or less.
- the minimum pore diameter of the meltblown nonwoven fabric is preferably 0.01 ⁇ m or more, more preferably 0.1 ⁇ m or more.
- the pore size (average pore size, maximum pore size, and minimum pore size) of the meltblown non-woven fabric can be measured by the bubble point method. Specifically, in accordance with JIS Z 8703: 1983 (standard state at the test site), a fluorine-based inert liquid (for example, It is impregnated with 3M, trade name: Florinert, and the pore size is measured with a capillary flow porometer (for example, Porous materials, Inc., product name: CFP-1200AE).
- a fluorine-based inert liquid for example, It is impregnated with 3M, trade name: Florinert
- a capillary flow porometer for example, Porous materials, Inc., product name: CFP-1200AE.
- the basis weight of the meltblown non-woven fabric can be determined depending on the application, but is usually 1 g / m 2 to 200 g / m 2 and preferably in the range of 2 g / m 2 to 150 g / m 2 .
- the porosity of the meltblown non-woven fabric is usually 40% or more, preferably in the range of 40% to 98%, and more preferably in the range of 60% to 95%.
- the porosity of the meltblown nonwoven fabric means the porosity at a location excluding the embossing point.
- the volume occupied by a portion having a porosity of 40% or more is preferably 90% or more, and it is more preferable to have a porosity of 40% or more in almost all portions.
- the meltblown non-woven fabric of the present disclosure is used for a filter, it is preferable that it is not embossed or not embossed in almost all areas. In the case of not being embossed, the pressure loss when fluid is allowed to pass through the filter is suppressed, and the filter channel length tends to be long, so the filtering performance tends to be improved.
- the melt-blown nonwoven fabric of this indication is laminated
- the air permeability of the meltblown non-woven fabric is preferably 3 cm 3 / cm 2 / sec to 30 cm 3 / cm 2 / sec, more preferably 5 cm 3 / cm 2 / sec to 20 cm 3 / cm 2 / sec, further preferably Is 8 cm 3 / cm 2 / sec to 12 cm 3 / cm 2 / sec.
- the meltblown non-woven fabric preferably contains no solvent component.
- the solvent component means an organic solvent component capable of dissolving the polypropylene polymer constituting the fiber.
- Examples of the solvent component include dimethylformamide (DMF) and the like.
- DMF dimethylformamide
- the absence of the solvent component means being below the detection limit by head space gas chromatography.
- the fibers of the meltblown non-woven fabric preferably have an entangled point at which the fibers are self-fused.
- the self-fused entanglement point means a branched portion where the fibers are bonded by fusing the polypropylene polymer itself constituting the fiber, and the entangled point formed by bonding the fibers via the binder resin. It is distinguished from The self-fused entanglement points are formed in the process of thinning the fibrous polypropylene polymer by meltblowing. Whether or not the fibers have a self-fusion-bonded entanglement point can be confirmed by an electron micrograph.
- the meltblown non-woven fabric having the entanglement points by self-fusion does not need to contain a resin component other than the polypropylene polymer constituting the fibers, and does not contain any resin component.
- the meltblown non-woven fabric may be used as a single-layer non-woven fabric or as a non-woven fabric constituting at least one layer of the non-woven fabric laminate.
- layers that make up the nonwoven laminate include conventional meltblown nonwovens, spunbonded nonwovens, other nonwovens such as needle punching and spunlaced nonwovens, as well as fabrics, knits, papers and the like.
- the nonwoven fabric laminate at least one melt-blown nonwoven fabric of the present disclosure may be contained, and two or more may be contained.
- other non-woven fabric, woven fabric, knitted fabric, paper and the like may be included as long as at least one of them is included, and two or more may be included.
- the nonwoven fabric laminate can be used as a filter, and may be used as a foam molding reinforcing material or the like.
- the meltblown non-woven fabric of the present disclosure may be used, for example, as a filter such as a gas filter (air filter) or a liquid filter.
- the meltblown non-woven fabric satisfies at least one of the following 1) to 3): 1) does not contain a solvent component, 2) does not contain an adhesive component for bonding fibers, and 3) is not embossed. In the case, the content of impurities is reduced. Therefore, such meltblown non-woven fabrics have high cleanliness and filtering performance, and are suitably used as high performance filters.
- the meltblown nonwoven fabric of the present disclosure can be suitably used as a liquid filter.
- the meltblown non-woven fabric of the present disclosure tends to have a small average fiber diameter and a large specific surface area. For this reason, it is preferable to use the meltblown non-woven fabric of the present disclosure as a liquid filter because it is excellent in particulate collection efficiency.
- the liquid filter may be comprised of a single layer of the meltblown nonwoven of the present disclosure or may be comprised of a nonwoven laminate of two or more layers of the meltblown nonwoven of the present disclosure.
- a nonwoven fabric laminate including two or more layers of meltblown nonwoven fabrics is used as the liquid filter, the two or more layers of meltblown nonwoven fabrics may be simply stacked.
- the liquid filter may combine the meltblown nonwoven of the present disclosure with other meltblown nonwovens depending on the purpose and the liquid to be applied.
- a spunbond nonwoven fabric, a mesh or the like may be laminated.
- the liquid filter may be calendered using, for example, a pair of flat rolls provided with a clearance between the flat rolls in order to control the hole diameter to be small.
- the clearances between the flat rolls need to be appropriately changed depending on the thickness of the non-woven fabric so that the gaps between the fibers of the non-woven fabric are eliminated.
- the roll surface temperature be thermally pressed in the range of 15 ° C. to 50 ° C. lower than the melting point of the polypropylene fiber.
- the roll surface temperature is lower by 15 ° C. or more than the melting point of the polypropylene fiber, the film formation of the surface of the meltblown non-woven fabric tends to be suppressed and the deterioration of the filter performance tends to be suppressed.
- the meltblown nonwoven fabric of the present disclosure may also be used as a foam molding reinforcing material.
- the reinforcing material for foam molding is, for example, a reinforcing material used to cover the surface of a foam molded product made of urethane or the like to protect the surface of the foam molded product or to enhance the rigidity of the foam molded product. It is.
- the reinforcing material for foam molding including the meltblown nonwoven fabric of the present disclosure is disposed on the inner surface of the mold for foam molding, and foam molding is performed to prevent the resin for foam such as urethane from exuding on the surface of the molded body. it can.
- a single-layer non-woven fabric consisting only of the meltblown non-woven fabric of the present disclosure may be used as a foam molding reinforcing material
- a non-woven fabric laminate in which a spunbond non-woven fabric is laminated on one side or both surfaces of the melt-blown non-woven fabric of the present disclosure is used. Is preferred. Lamination of the spunbond nonwoven fabric facilitates, for example, lamination with other layers.
- the spunbond non-woven fabric used for a foam molding reinforcing material preferably has a fiber diameter of 10 ⁇ m to 40 ⁇ m, more preferably 10 ⁇ m to 20 ⁇ m, and a fabric weight of 10 g / m 2 to 50 g / m 2 Preferably, it is 10 g / m 2 to 20 g / m 2 .
- the fiber diameter and the fabric weight of the spunbonded nonwoven fabric layer are in the above-mentioned range, it is easy to prevent the exudation of the foaming resin, and the weight reduction of the foam molding reinforcing material can be achieved.
- the reinforcing material for foam molding may further have a reinforcing layer or the like on the spunbond nonwoven fabric, as necessary.
- a reinforcing layer or the like on the spunbond nonwoven fabric, as necessary.
- Various well-known nonwoven fabrics etc. can be used as a reinforcement layer.
- the foam-forming reinforcing material has a reinforcing layer on only one side, the foam-forming reinforcing material is used by being disposed such that the reinforcing layer is closer to the foam resin than the meltblown non-woven fabric of the present disclosure.
- the method for producing the meltblown non-woven fabric of the present disclosure is not particularly limited, and conventionally known methods can be applied.
- the manufacturing method which has the following processes can be mentioned.
- the meltblown method is one of the fleece forming methods in the production of meltblown nonwovens.
- a polypropylene-based polymer as a raw material is melted using an extruder or the like.
- the molten polypropylene polymer is introduced into a spinneret connected to the tip of an extruder, and discharged in a fiber form from a spinning nozzle of the spinneret.
- a high temperature gas for example, air
- the extruded fibrous molten polypropylene polymer is drawn to a high temperature gas, and thus is refined to a diameter of usually 1.4 ⁇ m or less, preferably 1.0 ⁇ m or less.
- the fibrous molten polypropylene polymer is reduced to the limit of high temperature gas.
- a high voltage may be applied to the narrowed fibrous molten polypropylene-based unit to further narrow it.
- a high voltage When a high voltage is applied, the fibrous molten polypropylene polymer is pulled toward the collecting side by the attractive force of the electric field and becomes thin.
- the voltage to be applied is not particularly limited, and may be 1 kV to 300 kV.
- the fibrous molten polypropylene polymer may be further thinned by irradiating it with a heat ray.
- a heat ray By irradiation with a heat ray, it is possible to thin and refine the flowability of the fibrous polypropylene polymer.
- the melt viscosity of the fibrous polypropylene polymer can be further lowered by irradiating a heat ray. Therefore, even if a polypropylene polymer having a large molecular weight is used as a spinning material, it is possible to obtain sufficiently thinned fibers, and a high strength meltblown nonwoven fabric can be obtained.
- the heat ray means an electromagnetic wave having a wavelength of 0.7 ⁇ m to 1000 ⁇ m, and particularly means a near infrared ray having a wavelength of 0.7 ⁇ m to 2.5 ⁇ m.
- the strength and the irradiation amount of the heat ray are not particularly limited as long as the fibrous molten polypropylene polymer is remelted.
- a near infrared lamp or near infrared heater of 1 V to 200 V, preferably 1 V to 20 V can be used.
- the fibrous molten polypropylene polymer is collected in the form of a web. Generally, it is collected and deposited by a collector. This produces a meltblown nonwoven.
- collectors include perforated belts, perforated drums and the like. Also, the collector may have an air collection portion, which may facilitate the collection of fibers.
- the fibers may be collected in the form of a web on a desired substrate previously provided on the collector.
- a desired substrate previously provided on the collector.
- previously provided substrates include meltblown nonwovens, spunbonded nonwovens, other nonwovens such as needle punching and spunlaced nonwovens, as well as fabrics, knits, papers and the like.
- meltblown nonwoven laminate used for high performance filters, wipers, etc. can also be obtained.
- the manufacturing apparatus for producing the meltblown nonwoven fabric of the present disclosure is not particularly limited as long as the meltblown nonwoven fabric of the present disclosure can be produced.
- An extruder which melts and conveys a polypropylene polymer 2) A spinneret for discharging the molten polypropylene polymer conveyed from the extruder into a fibrous form, 3) A gas nozzle for injecting high temperature gas at the lower part of the spinneret, 4) A collector for collecting the fibrous molten polypropylene polymer discharged from the spinneret in the form of a web, And manufacturing equipment.
- the extruder is not particularly limited, and may be a single-screw extruder or a multi-screw extruder.
- the solid polypropylene polymer introduced from the hopper is melted in the compression section.
- the spinneret is located at the tip of the extruder.
- a spinneret usually comprises a plurality of spinning nozzles, for example, a plurality of spinning nozzles arranged in a row.
- the diameter of the spinning nozzle is preferably 0.05 mm to 0.38 mm.
- the molten polypropylene polymer is conveyed by the extruder to the spinneret and introduced into the spinning nozzle.
- a fibrous molten polypropylene polymer is discharged from the opening of the spinning nozzle.
- the discharge pressure of the molten polypropylene polymer is usually in the range of 0.01 kg / cm 2 to 200 kg / cm 2 , and preferably in the range of 10 kg / cm 2 to 30 kg / cm 2 .
- the discharge amount is increased more than this to realize mass production.
- the gas nozzle injects a high temperature gas in the lower part of the spinneret, more specifically near the opening of the spinning nozzle.
- the propellant gas may be air.
- a gas nozzle is provided in the vicinity of the opening of the spinning nozzle, and a high temperature gas is injected to the polypropylene polymer immediately after the discharge from the nozzle opening.
- the speed (discharge air volume) of the gas to be injected is not particularly limited, and may be 4 N mm 3 / min / m to 30 N mm 3 / min / m.
- the temperature of the injected gas is usually 5 ° C. to 400 ° C. or less, preferably in the range of 250 ° C. to 350 ° C.
- the type of gas to be injected is not particularly limited, and compressed air may be used.
- the meltblown non-woven fabric manufacturing apparatus may further comprise a voltage applying means for applying a voltage to the fibrous molten polypropylene polymer discharged from the spinneret.
- heat ray irradiation means for irradiating a heat ray to the fibrous molten polypropylene polymer discharged from the spinneret may further be provided.
- the collector for collecting in the form of a web is not particularly limited, and, for example, fibers may be collected on a porous belt.
- the mesh width of the porous belt is preferably 5 mesh to 200 mesh.
- an air collection unit may be provided on the back side of the fiber collection surface of the porous belt to facilitate collection.
- the distance from the collection surface of the collector to the nozzle opening of the spinning nozzle is preferably 3 cm to 55 cm.
- Peak Fiber Diameter Ratio The average fiber diameter and the peak fiber diameter in the fiber diameter distribution were measured, and the obtained peak fiber diameter was divided by the average fiber diameter. The measurement method of the average fiber diameter and the peak fiber diameter in fiber diameter distribution was performed as follows.
- the value of the geometric average of the minimum value and the maximum value of the x axis in the divided section was taken as the peak fiber diameter (mode fiber diameter).
- Example 1 85 parts by mass of Achieve 6936G2 (product name, manufactured by ExxonMobil, weight-average molecular weight: 550,000 propylene polymer, MFR: 1550) as high molecular weight propylene polymer A and high as low molecular weight propylene polymer B 15 parts by mass of wax NP055 (product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 7700 propylene polymer) was mixed to obtain 100 parts by mass of a propylene-based polymer mixture (1).
- Achieve 6936G2 product name, manufactured by ExxonMobil, weight-average molecular weight: 550,000 propylene polymer, MFR: 1550
- wax NP055 product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 7700 propylene polymer
- the measurement of the propylene-based polymer mixture (1) by GPC according to the above-mentioned method revealed that peak tops were present at a position of 55,000 molecular weight and a position of 8,000 molecular weight. The number of peak tops was two.
- the weight average molecular weight (Mw) of the propylene-based polymer mixture (1) was 38,000.
- the intrinsic viscosity [(] of the propylene-based polymer mixture (1) was measured by the method described above, and was 0.56 (dl / g).
- the GPC chart of the propylene-based polymer mixture (1) is shown in FIG.
- Propylene-based polymer mixture (1) is supplied to a die, and is discharged together with heated air (280 ° C., 120 m / sec) blown out from both sides of the nozzle at 50 mg / min. A meltblown nonwoven was obtained.
- the diameter of the die nozzle was 0.12 mm.
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio and specific surface area of the obtained meltblown nonwoven fabric were measured by the above-mentioned method. The results are shown in Table 1.
- the obtained melt-blown nonwoven fabric was subjected to GPC measurement by the method described above.
- the obtained GPC chart is shown in FIG.
- peak tops were present at a position of 55,000 molecular weight and at a position of 8,000 molecular weight.
- the number of peak tops was two.
- the weight average molecular weight (Mw) of the meltblown nonwoven fabric was 38,000.
- Example 2 In Example 1, in place of 100 parts by mass of the propylene-based polymer mixture (1), Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000) as a high molecular weight propylene-based polymer A Mixture of 90 parts by mass of a polymer, MFR: 1550) and 10 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) as a low molecular weight propylene polymer B The same operation as in Example 1 was performed except that 100 parts by mass of the propylene-based polymer mixture (2) was used.
- 6936G2 product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000
- Hi-Wax NP 055 product name,
- the measurement of the propylene-based polymer mixture (2) by GPC according to the method described above revealed that peak tops were present at positions of 55,000 molecular weight and 8,000 molecular weight. The number of peak tops was two.
- the weight average molecular weight (Mw) of the propylene-based polymer mixture (2) was 53,000.
- the intrinsic viscosity [(] of the propylene-based polymer mixture (2) was measured by the above-mentioned method, and it was 0.56 (dl / g).
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- Example 1 In place of 100 parts by mass of the propylene-based polymer mixture (1), Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000) as a high molecular weight propylene-based polymer A The same operation as in Example 1 was performed except that 100 parts by mass of the polymer, MFR: 1550) alone was used.
- Achieve 6936G2 as the high molecular weight polypropylene polymer A was measured by GPC according to the method described above, a peak top was present only at a position of 55,000 in molecular weight.
- the limiting viscosity [ ⁇ ] of Achieve 6936G2 as the high molecular weight propylene polymer A was measured by the method described above and found to be 0.63 (dl / g).
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- Example 2 instead of 100 parts by mass of the propylene-based polymer mixture (1), 650Y as a high molecular weight propylene-based polymer A (product name, manufactured by Polymire, a propylene-based weight having a weight average molecular weight of 51,000) The same operation as in Example 1 was carried out except that 100 parts by mass of the combined, MFR: 1800) was used alone.
- 650Y as high molecular weight polypropylene polymer A was measured by GPC according to the above-mentioned method, a peak top was present only at the position of 51,000 molecular weight.
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- Example 3 In Example 1, 94 parts by mass of Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550) instead of 100 parts by mass of a propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (3) which is a mixture of 6 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
- Achieve 6936G2 product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550
- Example 1 except using 100 parts by mass of a propylene-based polymer mixture (3) which is a mixture of 6 parts by mass of Hi-Wax NP 05
- the measurement of the propylene-based polymer mixture (3) by GPC according to the above-mentioned method revealed that a peak top was present only at a position of 55,000 in molecular weight.
- the weight average molecular weight of the propylene-based polymer mixture (3) was 54,000.
- the intrinsic viscosity [ ⁇ ⁇ ⁇ ⁇ ⁇ ] of the propylene-based polymer mixture (3) was measured by the method described above, and was 0.59 (dl / g).
- the GPC chart of the propylene-based polymer mixture (3) is shown in FIG.
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- Example 4 In Example 1, 50 parts by weight of Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550) instead of 100 parts by weight of a propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (4) which is a mixture of 50 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
- Achieve 6936G2 product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550
- Example 1 except using 100 parts by mass of a propylene-based polymer mixture (4) which is a mixture of 50 parts by mass of Hi-Wax NP
- the measurement of the propylene-based polymer mixture (4) by GPC according to the above-mentioned method revealed that peak tops were present at a weight-average molecular weight of 55,000 and a molecular weight of 8,000. The number of peak tops was two. The weight average molecular weight of the propylene-based polymer mixture (4) was 29,000. Further, the intrinsic viscosity [(] of the propylene-based polymer mixture (4) was measured by the above-mentioned method and found to be 0.41 (dl / g).
- Example 1 85 parts by mass of S119 (product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 1710,000 propylene-based polymer, MFR: 60) instead of 100 parts by mass of the propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (5) which is a mixture of 15 parts by mass of High Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
- S119 product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 1710,000 propylene-based polymer, MFR: 60
- Example 1 except using 100 parts by mass of a propylene-based polymer mixture (5) which is a mixture of 15 parts by mass of High Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-
- the measurement of the propylene-based polymer mixture (5) by GPC according to the above-mentioned method revealed that peak tops were present at positions of a molecular weight of 170,000 and a molecular weight of 8,000. The number of peak tops was two. The weight average molecular weight of the propylene-based polymer mixture (5) was 162,000. Further, the intrinsic viscosity [[] of the propylene-based polymer mixture (4) was measured by the method described above, to be 1.2 (dl / g). The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- Example 6 instead of 100 parts by mass of a propylene-based polymer mixture, SP50500P (product name, manufactured by Prime Polymer Co., Ltd., ethylene-based polymer having a weight average molecular weight of 38,000, in accordance with JIS K 7210-1: 2014 And a mixture of 85 parts by weight of MFR measured at 190 ° C. under a load of 2.16 kg and 15 parts by weight of Hi-Wax 720P (product name, Mitsui Chemicals, Inc., ethylene-based polymer with a weight average molecular weight of 7000) The same operation as in Example 1 was performed except that 100 parts by mass of the ethylene-based polymer mixture was used.
- SP50500P product name, manufactured by Prime Polymer Co., Ltd., ethylene-based polymer having a weight average molecular weight of 38,000, in accordance with JIS K 7210-1: 2014
- Hi-Wax 720P product name, Mitsui Chemicals, Inc., ethylene-based polymer with
- the ethylene-based polymer mixture was measured by GPC according to the above-mentioned method, no peak top derived from a propylene-based polymer was present.
- the peak top derived from the ethylene-based polymer was present at a molecular weight of 38,000 and a molecular weight of 7,000.
- the weight average molecular weight of the ethylene-based polymer mixture was 31,000.
- the intrinsic viscosity [(] of the ethylene-based polymer mixture was measured by the above-mentioned method to be 0.61 (dl / g).
- the average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [ ⁇ ] of the obtained meltblown nonwoven fabric are shown in Table 1.
- PP represents polypropylene and PE represents polyethylene.
- the average fiber diameter is smaller and the specific surface area is larger than that of the meltblown nonwoven fabric of the comparative example. For this reason, when the meltblown nonwoven fabric of an Example is used as a filter, it turns out that it is excellent in the collection efficiency of microparticles.
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Abstract
Description
不織布を構成する繊維としては、ポリプロピレンやポリエチレンなどの熱可塑性樹脂の繊維が知られている。 A non-woven fabric (also referred to as a melt-blown non-woven fabric or a melt-blown non-woven fabric) produced by the melt-blowing method is superior in flexibility, uniformity and compactness because it can thin fibers constituting the non-woven fabric compared with general spunbonded non-woven fabrics. ing. For this reason, the meltblown non-woven fabric is laminated alone or with other non-woven fabric, etc., and filters such as liquid filters and air filters, sanitary materials, medical materials, agricultural coating materials, civil engineering materials, building materials, oil adsorbents, automobile materials , Electronic materials, separators, clothes, packaging materials, etc.
As a fiber which comprises a nonwoven fabric, the fiber of thermoplastic resins, such as a polypropylene and polyethylene, is known.
また、特許文献4及び特許文献5に記載された製造方法は、特別な装置を用いており、通常のメルトブローン法よりも生産速度が遅いことがわかった。
そこで、本発明では、通常のメルトブローン法で製造でき、かつ、捕集効率に優れる、すなわち平均繊維径が小さく、比表面積が大きい不織布、及び該不織布を用いたフィルタを提供することを課題とする。 The inventors of the present invention have found that the nonwoven fabrics described in
Moreover, the manufacturing method described in patent document 4 and patent document 5 uses a special apparatus, and it turned out that production speed is slower than the usual meltblown method.
Therefore, in the present invention, it is an object of the present invention to provide a non-woven fabric which can be manufactured by the usual melt-blowing method and is excellent in collection efficiency, that is, a small average fiber diameter and a large specific surface area, and a filter using the non-woven fabric. .
<1> ゲルパーミエーションクロマトグラフィーにおける排出曲線において、分子量2万以上の位置に少なくとも1つのピークトップと、分子量2万未満の位置に少なくとも1つのピークトップとを有し、極限粘度[η]が0.50(dl/g)~0.75(dl/g)であるプロピレン系重合体からなるメルトブローン不織布。
<2> 前記プロピレン系重合体は、重量平均分子量が2万以上である高分子量プロピレン系重合体Aと、重量平均分子量が2万未満である低分子量プロピレン系重合体Bとを少なくとも含む<1>に記載のメルトブローン不織布。
<3> 前記プロピレン系重合体の全質量に対する前記低分子量プロピレン系重合体Bの含有率が、8質量%~40質量%である<2>に記載のメルトブローン不織布。
<4> 前記プロピレン系重合体の全質量に対する前記高分子量プロピレン系重合体Aの含有率が、60質量%~92質量%である<2>又は<3>に記載のメルトブローン不織布。
<5> 前記高分子量プロピレン系重合体Aのメルトフローレート(MFR)が、1000g/10分~2500g/10分である<2>~<4>のいずれか1項に記載のメルトブローン不織布。
<6> 前記プロピレン系重合体の重量平均分子量は、2万以上である<1>~<5>のいずれか1項に記載のメルトブローン不織布。
<7> 平均繊維径が1.1μm未満の繊維で構成される<1>~<6>のいずれか1項に記載のメルトブローン不織布。
<8> 比表面積が2.0m2/g~20.0m2/gである<1>~<7>のいずれか1項に記載のメルトブローン不織布。
<9> 平均繊維径に対するピーク繊維径の比率が0.5を超える<1>~<8>のいずれか1項に記載のメルトブローン不織布。
<10> <1>~<9>のいずれか1項に記載のメルトブローン不織布を少なくとも含む不織布積層体。
<11> <1>~<9>のいずれか1項に記載のメルトブローン不織布を含むフィルタ。
<12> 液体用フィルタである<11>に記載のフィルタ。 The means for solving the above-mentioned subject are as follows.
<1> In the discharge curve in gel permeation chromatography, it has at least one peak top at a molecular weight of 20,000 or more and at least one peak top at a position of molecular weight less than 20,000, and the intrinsic viscosity [η] is A meltblown non-woven fabric comprising a propylene-based polymer of 0.50 (dl / g) to 0.75 (dl / g).
<2> The propylene-based polymer includes at least a high molecular weight propylene-based polymer A having a weight average molecular weight of 20,000 or more and a low molecular weight propylene-based polymer B having a weight average molecular weight of less than 20,000. The meltblown nonwoven fabric as described in>.
<3> The meltblown nonwoven fabric according to <2>, wherein a content of the low molecular weight propylene polymer B with respect to a total mass of the propylene polymer is 8% by mass to 40% by mass.
<4> The meltblown nonwoven fabric according to <2> or <3>, wherein the content of the high molecular weight propylene polymer A is 60% by mass to 92% by mass with respect to the total mass of the propylene polymer.
<5> The meltblown nonwoven fabric according to any one of <2> to <4>, wherein a melt flow rate (MFR) of the high molecular weight propylene polymer A is 1000 g / 10 minutes to 2500 g / 10 minutes.
<6> The meltblown nonwoven fabric according to any one of <1> to <5>, wherein the weight average molecular weight of the propylene-based polymer is 20,000 or more.
<7> The meltblown nonwoven fabric according to any one of <1> to <6>, which is composed of fibers having an average fiber diameter of less than 1.1 μm.
<8> a specific surface area of 2.0m 2 /g~20.0m 2 / g <1 > ~ meltblown nonwoven fabric according to any one of <7>.
The melt-blown non-woven fabric according to any one of <1> to <8>, wherein the ratio of the peak fiber diameter to the average fiber diameter is more than 0.5.
<10> A nonwoven fabric laminate including at least the meltblown nonwoven fabric according to any one of <1> to <9>.
<11> A filter comprising the meltblown nonwoven fabric according to any one of <1> to <9>.
<12> The filter according to <11>, which is a filter for liquid.
本開示のメルトブローン不織布は、プロピレン系重合体からなる。本開示において、プロピレン系重合体とは、プロピレンの含有率が50質量%以上の重合体をいう。 <Propylene-based polymer>
The meltblown nonwoven fabric of the present disclosure comprises a propylene-based polymer. In the present disclosure, a propylene-based polymer refers to a polymer having a propylene content of 50% by mass or more.
なお、高分子側ピークトップおよび低分子側ピークトップの数は、プロピレン系重合体に由来するピークトップのみを数えればよい。 The propylene-based polymer has at least one peak top at a molecular weight of 20,000 or more and at least one peak top at a molecular weight less than 20,000 in an emission curve in GPC. Hereinafter, a peak top appearing at a position of a molecular weight of 20,000 or more in the discharge curve of GPC will be referred to as "polymer side peak top", and a peak top appearing at a position of molecular weight less than 20,000 will be referred to as "low molecular side peak top".
In addition, the number of the polymer side peak tops and the number of low molecular side peak tops may be calculated by counting only the peak tops derived from the propylene-based polymer.
高分子側ピークトップの少なくとも1つは、分子量2万~8万の範囲に位置することが好ましく、3万~7万の範囲に位置することが好ましく、4万~6.5万の範囲に位置することがより好ましい。上記範囲内であると、平均繊維径が小さくなる傾向にあるため好ましい。 At least one of the polymer-side peak tops is located at a molecular weight of 20,000 or more, preferably 30,000 or more, and more preferably 40,000 or more.
Preferably, at least one of the polymer side peak tops is located in the range of 20,000 to 80,000, preferably in the range of 30,000 to 70,000, and in the range of 40,000 to 65,000. It is more preferred to be located. Within the above range, the average fiber diameter tends to be small, which is preferable.
低分子側ピークトップの少なくとも1つは、分子量400以上2万未満の範囲に位置することが好ましく、400~1.5万の範囲に位置することが好ましく、1000~1.4万の範囲に位置することがより好ましく、2000~1.3万の範囲に位置することがさらに好ましく、6000~1.3万の範囲に位置することが特に好ましい。上記範囲内であると、紡糸中の繊維切れが起こりづらく紡糸性が高いままで、平均繊維径を小さくできる傾向にあるため好ましい。 At least one of the low molecular weight side peak tops is located at a molecular weight less than 20,000, preferably at 15,000 or less, more preferably at 14,000 or less, and 13,000 or less It is further preferred to be located.
Preferably, at least one of the low molecular weight side peak tops is located in the range of molecular weight 400 to less than 20,000, preferably in the range of 400 to 15,000, and in the range of 1000 to 14,000. It is more preferably located, more preferably in the range of 2000 to 13,000, and particularly preferably in the range of 6000 to 13,000. Within the above range, fiber breakage during spinning hardly occurs and the spinnability remains high, and the average fiber diameter tends to be reduced, which is preferable.
カラム :TOSO GMHHR-H(S)HT
検出器 :液体クロマトグラム用RI検出器 WATERS 150C [GPC measuring device]
Column: TOSO GMHHR-H (S) HT
Detector: RI detector for liquid chromatography WATERS 150C
溶媒 :1,2,4-トリクロロベンゼン
測定温度 :145℃
流速 :1.0ml/分
試料濃度 :2.2mg/ml
注入量 :160μl
検量線 :Universal Calibration
解析プログラム:HT-GPC(Ver.1.0) [Measurement condition]
Solvent: 1,2,4-Trichlorobenzene Measurement temperature: 145 ° C
Flow rate: 1.0 ml / min Sample concentration: 2.2 mg / ml
Injection volume: 160 μl
Calibration curve: Universal Calibration
Analysis program: HT-GPC (Ver. 1.0)
紡糸不良の抑制と、平均繊維径及び比表面積の観点から、プロピレン系重合体の極限粘度[η]は、0.52(dl/g)~0.70(dl/g)であることが好ましく、0.55(dl/g)~0.60(dl/g)であることがより好ましい。 The intrinsic viscosity [η] of the propylene-based polymer is 0.50 (dl / g) to 0.75 (dl / g). If the intrinsic viscosity [η] is less than 0.50 (dl / g), spinning defects such as broken threads are likely to occur. When the intrinsic viscosity [η] exceeds 0.75 (dl / g), the average fiber diameter is large and the specific surface area is small, and the collection efficiency is poor.
The intrinsic viscosity [η] of the propylene-based polymer is preferably 0.52 (dl / g) to 0.70 (dl / g) from the viewpoint of suppression of spinning defects and the viewpoint of average fiber diameter and specific surface area. More preferably, it is 0.55 (dl / g) to 0.60 (dl / g).
プロピレン系重合体約20mgをデカリン15mlに溶解し、135℃のオイルバス中で比粘度ηspを測定する。このデカリン溶液にデカリン溶媒を5ml追加して希釈後、同様にして比粘度ηspを測定する。この希釈操作をさらに2回繰り返し、濃度(C)を0に外挿したときのηsp/Cの値を極限粘度として求める(下式参照)。
[η]=lim(ηsp/C) (C→0) The intrinsic viscosity [η] of the propylene-based polymer is a value measured at 135 ° C. using a decalin solvent. Specifically, it is determined as follows.
About 20 mg of a propylene-based polymer is dissolved in 15 ml of decalin, and the specific viscosity sp sp is measured in an oil bath at 135 ° C. After diluting 5 ml of a decalin solvent to the decalin solution to dilute, the specific viscosity sp sp is measured in the same manner. This dilution operation is further repeated twice, and the value of spsp / C when the concentration (C) is extrapolated to 0 is determined as the limiting viscosity (see the following equation).
[Η] = lim (ηsp / C) (C → 0)
プロピレン系重合体におけるプロピレンの含有率が上記範囲内であると、後述する高分子量ポリプロピレン系重合体Aと、後述する低分子量ポリプロピレン系重合体Bとを含む場合に、相溶性に優れ、紡糸性が向上し、平均繊維径がより小さくなる傾向にあり好ましい。 The propylene-based polymer preferably has a propylene content of 70% by mass or more, more preferably 80% by mass or more, still more preferably 90% by mass or more, and a propylene homopolymer Is particularly preferred.
When the content of propylene in the propylene-based polymer is within the above range, the compatibility is excellent when the high molecular weight polypropylene polymer A described later and the low molecular weight polypropylene polymer B described later are included, and the spinnability is excellent. And the average fiber diameter tends to be smaller, which is preferable.
また、GPCの排出曲線において分子量2万以上と分子量2万未満のそれぞれの位置にピークトップを有するプロピレン系重合体は、多段重合を実施し、触媒化合物の種類や多段重合の段数などを適宜調整して調製してもよい。 The propylene-based polymer having a peak top at each position of a molecular weight of 20,000 or more and a molecular weight less than 20,000 in the discharge curve of GPC is at least one of high molecular weight propylene-based polymer A having Mw of 20,000 or more, and Mw is It may be prepared by including at least one low molecular weight propylene polymer B which is less than 20,000. That is, it may be a mixture of the high molecular weight propylene polymer A and the low molecular weight propylene polymer B (hereinafter, also referred to as a “propylene polymer mixture”).
In addition, a propylene-based polymer having a peak top at each position of a molecular weight of 20,000 or more and a molecular weight of less than 20,000 in the discharge curve of GPC carries out multi-stage polymerization, and appropriately adjusts the type of catalyst compound, number of stages of multi-stage polymerization, etc. It may be prepared.
高分子量プロピレン系重合体Aは、Mwが2万以上であり、3万以上であることが好ましく、4万以上であることがより好ましい。
また、高分子量プロピレン系重合体AのMwは、8万以下であることが好ましく、7万以下であることがより好ましく、6.5万以下であることがさらに好ましい。
上記範囲内であると、平均繊維径が小さくなる傾向にあるため好ましい。 <High molecular weight propylene polymer A>
The Mw of the high molecular weight propylene polymer A is 20,000 or more, preferably 30,000 or more, and more preferably 40,000 or more.
The Mw of the high molecular weight propylene polymer A is preferably 80,000 or less, more preferably 70,000 or less, and still more preferably 65,000 or less.
Within the above range, the average fiber diameter tends to be small, which is preferable.
また、高分子量プロピレン系重合体Aは、一種を単独で用いても、二種以上を併用してもよい。 The high molecular weight propylene polymer A may be a homopolymer of propylene or a copolymer of propylene and an α-olefin. Examples of copolymerized α-olefins are as described above. From the viewpoint of high compatibility with the low molecular weight polypropylene polymer B, the high molecular weight propylene polymer A preferably has a propylene content of 70% by mass or more, and more preferably 80% by mass or more. It is more preferable that it is 90 mass% or more, and it is especially preferable that it is a propylene homopolymer. When the compatibility is excellent, the spinnability is improved, and the average fiber diameter tends to be smaller, which is preferable.
The high molecular weight propylene polymer A may be used alone or in combination of two or more.
高分子量プロピレン系重合体Aの含有率が上記範囲の場合は、平均繊維径が小さくかつ比表面積が大きくなる傾向がある。また、紡糸性、繊維強度、微粒子の捕集効率、及び濾過流量のバランスに優れる傾向にある。
なお、プロピレン系重合体の全質量とは、全構成単位に対するプロピレンの含有率が50質量%以上の重合体の合計の質量を意味する。 The content of the high molecular weight propylene polymer A based on the total mass of the propylene polymer is preferably 60 mass% to 92 mass%, more preferably 62 mass% to 90 mass%, and 70 mass%. It is further preferable that the content is ~ 88% by mass.
When the content of the high molecular weight propylene polymer A is in the above range, the average fiber diameter tends to be small and the specific surface area tends to be large. In addition, the balance of spinnability, fiber strength, collection efficiency of fine particles, and filtration flow rate tends to be excellent.
In addition, the total mass of a propylene-type polymer means the mass of the sum total of the polymer whose content rate of propylene with respect to all the structural units is 50 mass% or more.
低分子量プロピレン系重合体Bは、Mwが2万未満であり、比較的分子量が低いため、ワックス状の重合体であってもよい。 <Low-molecular-weight propylene polymer B>
The low molecular weight propylene polymer B may be a wax-like polymer because the Mw is less than 20,000 and the molecular weight is relatively low.
また、低分子量プロピレン系重合体BのMwは、400以上であることが好ましく、1000以上であることがより好ましく、2000以上であることがさらに好ましく、6000以上であることが特に好ましい。
上記範囲内であると、紡糸中の繊維切れが起こりづらく紡糸性が高いままで、平均繊維径を小さくできる傾向にあるため好ましい。 The Mw of the low molecular weight propylene polymer B is preferably 15,000 or less, more preferably 14,000 or less, and still more preferably 13,000 or less.
The Mw of the low molecular weight propylene polymer B is preferably 400 or more, more preferably 1000 or more, still more preferably 2000 or more, and particularly preferably 6000 or more.
Within the above range, fiber breakage during spinning hardly occurs and the spinnability remains high, and the average fiber diameter tends to be reduced, which is preferable.
また、低分子量プロピレン系重合体Bは、一種を単独で用いても、二種以上を併用してもよい。 The low molecular weight propylene polymer B may be a homopolymer of propylene or a copolymer of propylene and an α-olefin. Examples of copolymerized α-olefins are as described above. From the viewpoint of excellent compatibility with the high molecular weight polypropylene polymer A, the low molecular weight propylene polymer B preferably has a propylene content of 70% by mass or more, and more preferably 80% by mass or more. It is more preferable that it is 90 mass% or more, and it is especially preferable that it is a propylene homopolymer. When the compatibility is excellent, the spinnability tends to be high, and the average fiber diameter tends to be smaller.
The low molecular weight propylene polymer B may be used alone or in combination of two or more.
低分子量プロピレン系重合体Bの軟化点が90℃を超えると、熱処理時又は使用時における耐熱安定性をより向上させることができ、結果としてフィルタ性能がより向上する傾向にある。低分子量プロピレン系重合体Bの軟化点の上限は特に制限されず、例えば、145℃が挙げられる。
本開示において、プロピレン系重合体の軟化点は、JIS K2207:2006に従って測定して得た値をいう。 The softening point of the low molecular weight propylene polymer B is preferably more than 90 ° C., and more preferably 100 ° C. or more.
When the softening point of the low molecular weight propylene polymer B exceeds 90 ° C., the heat resistance stability during heat treatment or use can be further improved, and as a result, the filter performance tends to be further improved. The upper limit of the softening point of the low molecular weight propylene polymer B is not particularly limited, and, for example, 145 ° C. may be mentioned.
In the present disclosure, the softening point of a propylene-based polymer refers to a value obtained by measuring according to JIS K 2207: 2006.
低分子量プロピレン系重合体Bの密度が上記範囲にあると、低分子量プロピレン系重合体Bと高分子量プロピレン系重合体Aとの混練性に優れ、且つ、紡糸性及び経時での安定性に優れる傾向にある。プロピレン系重合体の密度の測定方法は、上述のとおりである。 The density of the low molecular weight propylene polymer B is not particularly limited, for example, be a 0.890g / cm 3 ~ 0.980g / cm 3, preferably 0.910g / cm 3 ~ 0.980g / cm 3 deli, more preferably 0.920g / cm 3 ~ 0.980g / cm 3, more preferably from 0.940g / cm 3 ~ 0.980g / cm 3.
When the density of the low molecular weight propylene polymer B is in the above range, the kneadability of the low molecular weight propylene polymer B and the high molecular weight propylene polymer A is excellent, and the spinnability and stability over time are excellent. There is a tendency. The method of measuring the density of the propylene-based polymer is as described above.
低分子量プロピレン系重合体Bの含有率が上記範囲の場合は、平均繊維径が小さくかつ比表面積が大きくなる傾向がある。また、紡糸性、繊維強度、微粒子の捕集効率、及び濾過流量のバランスに優れる傾向にある。
なお、プロピレン系重合体の全質量とは、全構成単位に対するプロピレンの含有率が50質量%以上の重合体の合計の質量を意味する。 The content of the low molecular weight propylene polymer B with respect to the total mass of the propylene polymer is preferably 8 mass% to 40 mass%, more preferably 10 mass% to 38 mass%, and 12 mass%. It is more preferable that the content be 30% by mass.
When the content of the low molecular weight propylene polymer B is in the above range, the average fiber diameter tends to be small and the specific surface area tends to be large. In addition, the balance of spinnability, fiber strength, collection efficiency of fine particles, and filtration flow rate tends to be excellent.
In addition, the total mass of a propylene-type polymer means the mass of the sum total of the polymer whose content rate of propylene with respect to all the structural units is 50 mass% or more.
メルトブローン不織布を構成する繊維の平均繊維径は、1.1μm未満であることが好ましく、0.3μm~1.0μmであることがより好ましく、0.5μm~0.9μmであることがさらに好ましい。本開示のプロピレン系重合体を用いることで、平均繊維径をより小さくすることが可能である。
メルトブローン不織布の平均繊維径は、メルトブローン不織布の電子顕微鏡写真(倍率1000倍)から、任意の100本の不織布繊維を選択し、選択した繊維の直径を測定し、その平均値をいう。 <Melt blown nonwoven>
The average fiber diameter of the fibers constituting the meltblown non-woven fabric is preferably less than 1.1 μm, more preferably 0.3 μm to 1.0 μm, and still more preferably 0.5 μm to 0.9 μm. By using the propylene-based polymer of the present disclosure, it is possible to make the average fiber diameter smaller.
The average fiber diameter of the meltblown non-woven fabric is an electron micrograph (magnification of 1000 times) of the meltblown non-woven fabric, 100 arbitrary non-woven fibers are selected, the diameter of the selected fibers is measured, and the average value is said.
ピーク繊維径比率は、0.53以上であることがより好ましく、0.55以上であることがさらに好ましい。ピーク繊維径比率の上限値は特に限定されず、例えば、0.95以下であってもよく、0.90以下であってもよい。 The meltblown non-woven fabric preferably has a ratio of peak fiber diameter to average fiber diameter (hereinafter also referred to as “peak fiber diameter ratio”) exceeds 0.5 when the fiber diameter distribution is measured. When the peak fiber diameter ratio exceeds 0.5, the fiber diameter distribution is narrowed, and the fiber diameter is made more uniform. Therefore, the generation of gaps caused by the non-uniform fiber diameter is suppressed, and the particle capture efficiency tends to be further improved.
The peak fiber diameter ratio is more preferably 0.53 or more, further preferably 0.55 or more. The upper limit of the peak fiber diameter ratio is not particularly limited, and may be, for example, 0.95 or less, or 0.90 or less.
(1)平均繊維径の測定
メルトブローン不織布を、株式会社日立製作所製電子顕微鏡「S-3500N」を用いて倍率5000倍の写真を撮影し、無作為に繊維の幅(直径:μm)を1000点測定し、数平均で平均繊維径(μm)を算出する。
メルトブローン不織布における繊維の測定箇所を無作為とするため、撮影した写真の左上隅から右下隅に対角線を引き、対角線と繊維が交差した箇所の繊維の幅(直径)を測定する。測定点が1000点となるまで新規に写真を撮影し測定を行う。 The measuring method of the average fiber diameter and peak fiber diameter in fiber diameter distribution is demonstrated.
(1) Measurement of average fiber diameter A meltblown non-woven fabric was photographed at a magnification of 5000 times using an electron microscope "S-3500N" manufactured by Hitachi, Ltd., and the fiber width (diameter: μm) was randomly 1000 points. Measure and calculate the average fiber diameter (μm) by number average.
In order to randomize the measurement points of the fibers in the meltblown non-woven fabric, a diagonal line is drawn from the upper left corner to the lower right corner of the photographed photograph, and the width (diameter) of the fibers at the intersection of the diagonal line and the fibers is measured. Take a picture and measure it until the measurement point reaches 1000 points.
既述の「(1)平均繊維径の測定方法」で測定された1000点の繊維径(μm)のデータに基づき、対数度数分布を作成する。
対数度数分布は、x軸を繊維径(μm)を、10を底とする対数スケール上にプロットし、y軸は頻度の百分率とする。x軸上において、繊維径0.1(=10-1)μmから、繊維径50.1(=101.7)μmまでを、対数スケール上で均等に27に分割し、頻度の最も大きい分割区間におけるx軸の最小値と最大値との相乗平均の値を、ピーク繊維径(最頻繊維径)とする。 (2) Peak fiber diameter (moderate fiber diameter)
Based on the data of the fiber diameter (μm) of 1000 points measured by the above-mentioned “(1) Measurement method of average fiber diameter”, logarithmic frequency distribution is created.
The logarithmic frequency distribution is plotted on a logarithmic scale with the x-axis as fiber diameter (μm) on the base of 10, and the y-axis is a percentage of the frequency. On the x-axis, the fiber diameter from 0.1 (= 10 -1 ) μm to the fiber diameter of 50.1 (= 10 1.7 ) μm is equally divided into 27 on a logarithmic scale, and the frequency is the largest The value of the geometric average of the minimum value and the maximum value of the x axis in the divided section is taken as the peak fiber diameter (mode diameter).
また、メルトブローン不織布の平均孔径は0.01μm以上であることが好ましく、0.1μm以上であることがより好ましい。平均孔径が0.01μm以上であると、メルトブローン不織布をフィルタに用いた場合に、圧損が抑えられ、流量を維持できる傾向にある。 The average pore diameter of the meltblown non-woven fabric is preferably 10.0 μm or less, more preferably 3.0 μm or less, and still more preferably 2.5 μm or less.
The average pore diameter of the meltblown non-woven fabric is preferably 0.01 μm or more, more preferably 0.1 μm or more. When a melt-blown non-woven fabric is used for a filter, when the average pore diameter is 0.01 μm or more, the pressure loss tends to be suppressed and the flow rate can be maintained.
また、メルトブローン不織布の最小孔径は、0.01μm以上であることが好ましく、0.1μm以上であることがより好ましい。 The maximum pore diameter of the meltblown nonwoven fabric is preferably 20 μm or less, more preferably 6.0 μm or less, and still more preferably 5.0 μm or less.
The minimum pore diameter of the meltblown nonwoven fabric is preferably 0.01 μm or more, more preferably 0.1 μm or more.
メルトブローン不織布の空隙率は、通常40%以上であり、40%~98%の範囲にあることが好ましく、60%~95%の範囲にあることがより好ましい。本開示のメルトブローン不織布がエンボス加工をされている場合には、メルトブローン不織布の空隙率は、エンボス点を除く箇所における空隙率を意味する。 The basis weight of the meltblown non-woven fabric can be determined depending on the application, but is usually 1 g / m 2 to 200 g / m 2 and preferably in the range of 2 g / m 2 to 150 g / m 2 .
The porosity of the meltblown non-woven fabric is usually 40% or more, preferably in the range of 40% to 98%, and more preferably in the range of 60% to 95%. When the meltblown nonwoven fabric of the present disclosure is embossed, the porosity of the meltblown nonwoven fabric means the porosity at a location excluding the embossing point.
本開示のメルトブローン不織布は、例えば、ガスフィルタ(エアフィルタ)、液体フィルタ等のフィルタとして用いてもよい。
メルトブローン不織布が、1)溶剤成分を含まず、2)繊維同士を接着させるための接着剤成分を含まず、3)エンボス加工が施されていない、これら1)~3)の少なくとも一つを満たす場合には、不純物の含有量が低減される。そのため、このようなメルトブローン不織布は、清浄性とフィルタリング性能が高く、高性能フィルタとして好適に用いられる。 <Use of meltblown non-woven fabric>
The meltblown non-woven fabric of the present disclosure may be used, for example, as a filter such as a gas filter (air filter) or a liquid filter.
The meltblown non-woven fabric satisfies at least one of the following 1) to 3): 1) does not contain a solvent component, 2) does not contain an adhesive component for bonding fibers, and 3) is not embossed. In the case, the content of impurities is reduced. Therefore, such meltblown non-woven fabrics have high cleanliness and filtering performance, and are suitably used as high performance filters.
本開示のメルトブローン不織布は、平均繊維径が小さく、かつ、比表面積が大きい傾向にある。このため、本開示のメルトブローン不織布を液体フィルタとして用いると、微粒子の捕集効率に優れるため好ましい。 The meltblown nonwoven fabric of the present disclosure can be suitably used as a liquid filter.
The meltblown non-woven fabric of the present disclosure tends to have a small average fiber diameter and a large specific surface area. For this reason, it is preferable to use the meltblown non-woven fabric of the present disclosure as a liquid filter because it is excellent in particulate collection efficiency.
また、液体用フィルタは、目的及び適用する液体に応じて、本開示のメルトブローン不織布に、他のメルトブローン不織布を組み合わせてもよい。また、液体用フィルタの強度を強めるために、スパンボンド不織布、網状物などを積層してもよい。 The liquid filter may be comprised of a single layer of the meltblown nonwoven of the present disclosure or may be comprised of a nonwoven laminate of two or more layers of the meltblown nonwoven of the present disclosure. When a nonwoven fabric laminate including two or more layers of meltblown nonwoven fabrics is used as the liquid filter, the two or more layers of meltblown nonwoven fabrics may be simply stacked.
Also, the liquid filter may combine the meltblown nonwoven of the present disclosure with other meltblown nonwovens depending on the purpose and the liquid to be applied. In addition, in order to increase the strength of the liquid filter, a spunbond nonwoven fabric, a mesh or the like may be laminated.
本開示のメルトブローン不織布の製造方法は特に制限されず、従来公知の方法を適用することができる。例えば、以下の工程を有する製造方法を挙げることができる。 <Method for producing meltblown non-woven fabric>
The method for producing the meltblown non-woven fabric of the present disclosure is not particularly limited, and conventionally known methods can be applied. For example, the manufacturing method which has the following processes can be mentioned.
2)繊維状ポリプロピレン系重合体を、ウェブ状に捕集する工程 1) A step of discharging a molten polypropylene polymer from a spinneret together with a heating gas by a meltblown method to obtain a fibrous polypropylene polymer 2) A step of collecting a fibrous polypropylene polymer in the form of a web
本開示のメルトブローン不織布を製造するための製造装置は、本開示のメルトブローン不織布を製造することができれば特に限定されない。例えば、
1)ポリプロピレン系重合体を溶融して搬送する押出機と、
2)押出機から搬送された溶融ポリプロピレン系重合体を、繊維状に吐出する紡糸口金と、
3)紡糸口金の下部に、高温ガスを噴射するガスノズルと、
4)紡糸口金から吐出された繊維状の溶融ポリプロピレン系重合体をウェブ状に捕集する捕集器と、
を具備する製造装置を挙げることができる。 <Meltblown non-woven fabric manufacturing equipment>
The manufacturing apparatus for producing the meltblown nonwoven fabric of the present disclosure is not particularly limited as long as the meltblown nonwoven fabric of the present disclosure can be produced. For example,
1) An extruder which melts and conveys a polypropylene polymer,
2) A spinneret for discharging the molten polypropylene polymer conveyed from the extruder into a fibrous form,
3) A gas nozzle for injecting high temperature gas at the lower part of the spinneret,
4) A collector for collecting the fibrous molten polypropylene polymer discharged from the spinneret in the form of a web,
And manufacturing equipment.
また、紡糸口金から吐出された繊維状の溶融ポリプロピレン系重合体に熱線を照射する熱線照射手段を、さらに具備してもよい。 The meltblown non-woven fabric manufacturing apparatus may further comprise a voltage applying means for applying a voltage to the fibrous molten polypropylene polymer discharged from the spinneret.
In addition, heat ray irradiation means for irradiating a heat ray to the fibrous molten polypropylene polymer discharged from the spinneret may further be provided.
本開示における全ての文献、特許出願、及び技術規格は、個々の文献、特許出願、及び技術規格が参照により取り込まれることが具体的かつ個々に記された場合と同程度に、本開示中に参照により取り込まれる。 The disclosure of Japanese Patent Application 2017-184520, filed on September 26, 2017, is incorporated by reference in its entirety.
All documents, patent applications and technical standards in the present disclosure may be incorporated into the present disclosure to the same extent as if each individual document, patent application and technical standard were specifically and individually incorporated by reference. Captured by reference.
実施例及び比較例における物性値等は、以下の方法により測定した。 Hereinafter, the present invention will be more specifically described based on examples, but the present invention is not limited to these examples.
Physical property values and the like in Examples and Comparative Examples were measured by the following methods.
メルトブローン不織布について、電子顕微鏡(株式会社日立製作所製S-3500N)を用いて、倍率1000倍の写真を撮影し、任意に繊維100本(n=100)を選び、その繊維の幅(直径)を測定し、得られた測定結果の平均を平均繊維径とした。 (1) Average fiber diameter For a meltblown non-woven fabric, a photograph of 1000 × magnification is taken using an electron microscope (S-3500N manufactured by Hitachi, Ltd.), 100 fibers (n = 100) are arbitrarily selected, and the fibers The width (diameter) of was measured, and the average of the obtained measurement results was taken as the average fiber diameter.
JIS Z8830:2013に準拠し、窒素ガスの物理吸着を用いた細孔分布計(Belsorp max、日本ベル株式会社製)により、メルトブローン不織布のBET比表面積(BET法による比表面積)(m2/g)を測定した。 (2) Specific surface area A BET specific surface area (specific surface area by BET method) of a meltblown non-woven fabric with a pore distribution meter (Belsorp max, manufactured by Nippon Bell Co., Ltd.) using physical adsorption of nitrogen gas according to JIS Z8830: 2013. (M 2 / g) was measured.
繊維径分布における平均繊維径とピーク繊維径を測定し、得られたピーク繊維径を平均繊維径で除した。繊維径分布における平均繊維径とピーク繊維径の測定方法は以下のようにして行った。 (3) Peak Fiber Diameter Ratio The average fiber diameter and the peak fiber diameter in the fiber diameter distribution were measured, and the obtained peak fiber diameter was divided by the average fiber diameter. The measurement method of the average fiber diameter and the peak fiber diameter in fiber diameter distribution was performed as follows.
メルトブローン不織布を、株式会社日立製作所製電子顕微鏡「S-3500N」を用いて倍率5000倍の写真を撮影し、無作為に繊維の幅(直径:μm)を1000点測定し、数平均で平均繊維径(μm)を算出した。
メルトブローン不織布における繊維の測定箇所を無作為とするため、撮影した写真の左上隅から右下隅に対角線を引き、対角線と繊維が交差した箇所の繊維の幅(直径)を測定する。測定点が1000点となるまで新規に写真を撮影し測定を行った。 (3-1) Average fiber diameter in fiber diameter distribution Meltblown non-woven fabric was photographed at a magnification of 5000 times using an electron microscope "S-3500N" manufactured by Hitachi, Ltd., and the fiber width (diameter: μm at random) 1000 points were measured, and the average fiber diameter (μm) was calculated by number average.
In order to randomize the measurement points of the fibers in the meltblown non-woven fabric, a diagonal line is drawn from the upper left corner to the lower right corner of the photographed photograph, and the width (diameter) of the fibers at the intersection of the diagonal line and the fibers is measured. A new photograph was taken and measured until the number of measurement points reached 1000.
既述の「(3-1)平均繊維径の測定方法」で測定された1000点の繊維径(μm)のデータに基づき、対数度数分布を作成した。
対数度数分布は、x軸を繊維径(μm)を、10を底とする対数スケール上にプロットし、y軸は頻度の百分率とした。x軸上において、繊維径0.1(=10-1)μmから、繊維径50.1(=101.7)μmまでを、対数スケール上で均等に27に分割し、頻度の最も大きい分割区間におけるx軸の最小値と最大値との相乗平均の値を、ピーク繊維径(最頻繊維径)とした。 (3-2) Peak fiber diameter in fiber diameter distribution (mode diameter)
The logarithmic frequency distribution was created based on the data of the fiber diameter (μm) of 1000 points measured by the “(3-1) Measuring method of average fiber diameter” described above.
The logarithmic frequency distribution is plotted on a logarithmic scale with the x-axis as fiber diameter (μm) on the base of 10, and the y-axis is a percentage of the frequency. On the x-axis, the fiber diameter from 0.1 (= 10 -1 ) μm to the fiber diameter of 50.1 (= 10 1.7 ) μm is equally divided into 27 on a logarithmic scale, and the frequency is the largest The value of the geometric average of the minimum value and the maximum value of the x axis in the divided section was taken as the peak fiber diameter (mode fiber diameter).
高分子量プロピレン系重合体AとしてAchieve 6936G2(製品名、ExxonMobil社製、重量平均分子量:5.5万のプロピレン系重合体、MFR:1550)85質量部と、低分子量プロピレン系重合体BとしてハイワックスNP055(製品名、三井化学株式会社製、重量平均分子量:7700のプロピレン系重合体)15質量部とを混合し、プロピレン系重合体混合物(1)の100質量部を得た。 Example 1
85 parts by mass of Achieve 6936G2 (product name, manufactured by ExxonMobil, weight-average molecular weight: 550,000 propylene polymer, MFR: 1550) as high molecular weight propylene polymer A and high as low molecular weight propylene polymer B 15 parts by mass of wax NP055 (product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 7700 propylene polymer) was mixed to obtain 100 parts by mass of a propylene-based polymer mixture (1).
プロピレン系重合体混合物(1)のGPCチャートを、図1に示す。 The measurement of the propylene-based polymer mixture (1) by GPC according to the above-mentioned method revealed that peak tops were present at a position of 55,000 molecular weight and a position of 8,000 molecular weight. The number of peak tops was two. The weight average molecular weight (Mw) of the propylene-based polymer mixture (1) was 38,000. Further, the intrinsic viscosity [(] of the propylene-based polymer mixture (1) was measured by the method described above, and was 0.56 (dl / g).
The GPC chart of the propylene-based polymer mixture (1) is shown in FIG.
メルトブローン不織布の約20mgをデカリン15mlに溶解し、135℃のオイルバス中で比粘度ηspを測定した。このデカリン溶液にデカリン溶媒を5ml追加して希釈後、同様にして比粘度ηspを測定した。この希釈操作をさらに2回繰り返し、濃度(C)を0に外挿したときのηsp/Cの値を極限粘度として求めた(下式参照)。
[η]=lim(ηsp/C) (C→0)
メルトブローン不織布の極限粘度[η]は、紡糸前と変わらず、0.56(dl/g)であった。 In addition, the intrinsic viscosity [η] of the obtained meltblown nonwoven fabric was measured by the following method.
About 20 mg of meltblown non-woven fabric was dissolved in 15 ml of decalin, and the specific viscosity sp sp was measured in an oil bath at 135 ° C. After diluting 5 ml of decalin solvent to the decalin solution to dilute, the specific viscosity sp sp was measured in the same manner. This dilution operation was further repeated twice, and the value of spsp / C when the concentration (C) was extrapolated to 0 was determined as the limiting viscosity (see the following equation).
[Η] = lim (ηsp / C) (C → 0)
The intrinsic viscosity [η] of the meltblown nonwoven fabric was 0.56 (dl / g), unchanged from that before spinning.
実施例1において、プロピレン系重合体混合物(1)100質量部の代わりに、高分子量プロピレン系重合体AとしてのAchieve 6936G2(製品名、ExxonMobil社製、重量平均分子量:5.5万のプロピレン系重合体、MFR:1550)90質量部と、低分子量プロピレン系重合体BとしてのハイワックスNP055(製品名、三井化学株式会社製、重量平均分子量7700のプロピレン系重合体)10質量部との混合物であるプロピレン系重合体混合物(2)100質量部を用いたこと以外は実施例1と同様の操作を行った。
プロピレン系重合体混合物(2)を前述の方法でGPCにて測定を実施したところ、分子量5万5千と分子量8千の位置にピークトップが存在した。ピークトップの数は2つであった。プロピレン系重合体混合物(2)の重量平均分子量(Mw)は5.3万であった。また、プロピレン系重合体混合物(2)の極限粘度[η]を前述の方法で測定したところ、0.56(dl/g)であった。得られたメルトブローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Example 2
In Example 1, in place of 100 parts by mass of the propylene-based polymer mixture (1), Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000) as a high molecular weight propylene-based polymer A Mixture of 90 parts by mass of a polymer, MFR: 1550) and 10 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) as a low molecular weight propylene polymer B The same operation as in Example 1 was performed except that 100 parts by mass of the propylene-based polymer mixture (2) was used.
The measurement of the propylene-based polymer mixture (2) by GPC according to the method described above revealed that peak tops were present at positions of 55,000 molecular weight and 8,000 molecular weight. The number of peak tops was two. The weight average molecular weight (Mw) of the propylene-based polymer mixture (2) was 53,000. Further, the intrinsic viscosity [(] of the propylene-based polymer mixture (2) was measured by the above-mentioned method, and it was 0.56 (dl / g). The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
実施例1において、プロピレン系重合体混合物(1)100質量部の代わりに、高分子量プロピレン系重合体AとしてのAchieve 6936G2(製品名、ExxonMobil社製、重量平均分子量:5.5万のプロピレン系重合体、MFR:1550)を単独で100質量部用いたこと以外は実施例1と同様の操作を行った。
高分子量ポリプロピレン系重合体AとしてのAchieve 6936G2を前述の方法でGPCにて測定を実施したところ、分子量5万5千の位置のみにピークトップが存在した。高分子量プロピレン系重合体AとしてのAchieve 6936G2の極限粘度[η]を前述の方法で測定したところ、0.63(dl/g)であった。得られたメルトブローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Comparative Example 1
In Example 1, in place of 100 parts by mass of the propylene-based polymer mixture (1), Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000) as a high molecular weight propylene-based polymer A The same operation as in Example 1 was performed except that 100 parts by mass of the polymer, MFR: 1550) alone was used.
When Achieve 6936G2 as the high molecular weight polypropylene polymer A was measured by GPC according to the method described above, a peak top was present only at a position of 55,000 in molecular weight. The limiting viscosity [η] of Achieve 6936G2 as the high molecular weight propylene polymer A was measured by the method described above and found to be 0.63 (dl / g). The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
実施例1において、プロピレン系重合体混合物(1)100質量部の代わりに、高分子量プロピレン系重合体Aとしての650Y(製品名、Polymire社製、重量平均分子量:5.1万のプロピレン系重合体、MFR:1800)を単独で100質量部用いたこと以外は実施例1と同様の操作を行った。高分子量ポリプロピレン系重合体Aとしての650Yを前述の方法でGPCにて測定を実施したところ、分子量5万1千の位置のみにピークトップが存在した。高分子量プロピレン系重合体Aとしての650Yの極限粘度[
η]を前述の方法で測定したところ、0.56(dl/g)であった。得られたメルトブ
ローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Comparative Example 2
In Example 1, instead of 100 parts by mass of the propylene-based polymer mixture (1), 650Y as a high molecular weight propylene-based polymer A (product name, manufactured by Polymire, a propylene-based weight having a weight average molecular weight of 51,000) The same operation as in Example 1 was carried out except that 100 parts by mass of the combined, MFR: 1800) was used alone. When 650Y as high molecular weight polypropylene polymer A was measured by GPC according to the above-mentioned method, a peak top was present only at the position of 51,000 molecular weight. Intrinsic viscosity of 650 Y as high molecular weight propylene polymer A [
It was 0.56 (dl / g) when eta] was measured by the above-mentioned method. The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
実施例1において、プロピレン系重合体混合物100質量部の代わりに、Achieve 6936G2(製品名、ExxonMobil社製、重量平均分子量:5.5万のプロピレン系重合体、MFR:1550)94質量部と、ハイワックスNP055(製品名、三井化学株式会社製、重量平均分子量7700のプロピレン系重合体)6質量部の混合物であるプロピレン系重合体混合物(3)100質量部を用いたこと以外は実施例1と同様の操作を行った。
プロピレン系重合体混合物(3)を前述の方法でGPCにて測定を実施したところ、分子量5万5千の位置のみにピークトップが存在した。プロピレン系重合体混合物(3)の重量平均分子量は5万4千であった。また、プロピレン系重合体混合物(3)の極限粘度[η]を前述の方法で測定したところ、0.59(dl/g)であった。
プロピレン系重合体混合物(3)のGPCチャートを、図1に示す。
得られたメルトブローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Comparative Example 3
In Example 1, 94 parts by mass of Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550) instead of 100 parts by mass of a propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (3) which is a mixture of 6 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
The measurement of the propylene-based polymer mixture (3) by GPC according to the above-mentioned method revealed that a peak top was present only at a position of 55,000 in molecular weight. The weight average molecular weight of the propylene-based polymer mixture (3) was 54,000. In addition, the intrinsic viscosity [プ ロ ピ レ ン] of the propylene-based polymer mixture (3) was measured by the method described above, and was 0.59 (dl / g).
The GPC chart of the propylene-based polymer mixture (3) is shown in FIG.
The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
実施例1において、プロピレン系重合体混合物100質量部の代わりに、Achieve 6936G2(製品名、ExxonMobil社製、重量平均分子量:5.5万のプロピレン系重合体、MFR:1550)50質量部と、ハイワックスNP055(製品名、三井化学株式会社製、重量平均分子量7700のプロピレン系重合体)50質量部の混合物であるプロピレン系重合体混合物(4)100質量部を用いたこと以外は実施例1と同様の操作を行った。
プロピレン系重合体混合物(4)を前述の方法でGPCにて測定を実施したところ、重量平均分子量5万5千と分子量8千の位置にピークトップが存在した。ピークトップの数は2つであった。プロピレン系重合体混合物(4)の重量平均分子量は2万9千であった。また、プロピレン系重合体混合物(4)の極限粘度[η]を前述の方法で測定したところ、0.41(dl/g)であった。 Comparative Example 4
In Example 1, 50 parts by weight of Achieve 6936G2 (product name, manufactured by ExxonMobil, a propylene-based polymer having a weight average molecular weight of 55,000, MFR: 1550) instead of 100 parts by weight of a propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (4) which is a mixture of 50 parts by mass of Hi-Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
The measurement of the propylene-based polymer mixture (4) by GPC according to the above-mentioned method revealed that peak tops were present at a weight-average molecular weight of 55,000 and a molecular weight of 8,000. The number of peak tops was two. The weight average molecular weight of the propylene-based polymer mixture (4) was 29,000. Further, the intrinsic viscosity [(] of the propylene-based polymer mixture (4) was measured by the above-mentioned method and found to be 0.41 (dl / g).
実施例1において、プロピレン系重合体混合物100質量部の代わりに、S119(製品名、三井化学社製、重量平均分子量:17.1万のプロピレン系重合体、MFR:60)85質量部と、ハイワックスNP055(製品名、三井化学株式会社製、重量平均分子量7700のプロピレン系重合体)15質量部の混合物であるプロピレン系重合体混合物(5)100質量部を用いたこと以外は実施例1と同様の操作を行った。
プロピレン系重合体混合物(5)を前述の方法でGPCにて測定を実施したところ、分子量17万と分子量8千の位置にピークトップが存在した。ピークトップの数は2つであった。プロピレン系重合体混合物(5)の重量平均分子量は16万2千であった。また、プロピレン系重合体混合物(4)の極限粘度[η]を前述の方法で測定したところ、1.2(dl/g)であった。得られたメルトブローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Comparative Example 5
In Example 1, 85 parts by mass of S119 (product name, manufactured by Mitsui Chemicals, Inc., weight-average molecular weight: 1710,000 propylene-based polymer, MFR: 60) instead of 100 parts by mass of the propylene-based polymer mixture, Example 1 except using 100 parts by mass of a propylene-based polymer mixture (5) which is a mixture of 15 parts by mass of High Wax NP 055 (product name, manufactured by Mitsui Chemicals, Inc., a propylene-based polymer having a weight average molecular weight of 7700) The same operation was performed.
The measurement of the propylene-based polymer mixture (5) by GPC according to the above-mentioned method revealed that peak tops were present at positions of a molecular weight of 170,000 and a molecular weight of 8,000. The number of peak tops was two. The weight average molecular weight of the propylene-based polymer mixture (5) was 162,000. Further, the intrinsic viscosity [[] of the propylene-based polymer mixture (4) was measured by the method described above, to be 1.2 (dl / g). The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
実施例1において、プロピレン系重合体混合物100質量部の代わりに、SP50500P(製品名、プライムポリマー社製、重量平均分子量:3.8万のエチレン系重合体、JIS K 7210-1:2014に準拠して190℃、荷重2.16kgで測定したMFR:135)85質量部と、ハイワックス720P(製品名、三井化学株式会社製、重量平均分子量:7000のエチレン系重合体)15質量部の混合物であるエチレン系重合体混合物100質量部を用いたこと以外は実施例1と同様の操作を行った。
エチレン系重合体混合物を前述の方法でGPCにて測定を実施したところ、プロピレン系重合体に由来するピークトップは存在しなかった。なお、エチレン系重合体に由来するピークトップは、分子量3万8千の位置と、分子量7千の位置に存在した。エチレン系重合体混合物の重量平均分子量は3万1千であった。また、エチレン系重合体混合物の極限粘度[η]を前述の方法で測定したところ、0.61(dl/g)であった。得られたメルトブローン不織布の平均繊維径、ピーク繊維径、ピーク繊維径比率、比表面積、及び極限粘度[η]を表1に示す。 Comparative Example 6
In Example 1, instead of 100 parts by mass of a propylene-based polymer mixture, SP50500P (product name, manufactured by Prime Polymer Co., Ltd., ethylene-based polymer having a weight average molecular weight of 38,000, in accordance with JIS K 7210-1: 2014 And a mixture of 85 parts by weight of MFR measured at 190 ° C. under a load of 2.16 kg and 15 parts by weight of Hi-Wax 720P (product name, Mitsui Chemicals, Inc., ethylene-based polymer with a weight average molecular weight of 7000) The same operation as in Example 1 was performed except that 100 parts by mass of the ethylene-based polymer mixture was used.
When the ethylene-based polymer mixture was measured by GPC according to the above-mentioned method, no peak top derived from a propylene-based polymer was present. The peak top derived from the ethylene-based polymer was present at a molecular weight of 38,000 and a molecular weight of 7,000. The weight average molecular weight of the ethylene-based polymer mixture was 31,000. Further, the intrinsic viscosity [(] of the ethylene-based polymer mixture was measured by the above-mentioned method to be 0.61 (dl / g). The average fiber diameter, peak fiber diameter, peak fiber diameter ratio, specific surface area, and intrinsic viscosity [η] of the obtained meltblown nonwoven fabric are shown in Table 1.
プロピレン・エチレン共重合体としてVistamaxxTM6202〔製品名、ExxonMobil社製、重量平均分子量:7万、MFR(230℃、2.16kg荷重):20g/10min、エチレン含量:15質量%〕40質量部と、プロピレン系重合体ワックス〔密度:0.900g/cm3、重量平均分子量:7800、軟化点148℃、エチレン含量:1.7質量%〕40質量部と、プロピレン単独重合体〔MFR:1500g/10分、重量平均分子量:54000〕20質量部と、を混合し、プロピレン系重合体組成物(6)を得た。 Comparative Example 7
Vistamaxx TM 6202 as propylene-ethylene copolymer [product name, ExxonMobil Corporation, weight average molecular weight: 70,000, MFR (230 ° C., 2.16 kg load): 20 g / 10min, ethylene content: 15 wt%] 40 parts by weight 40 parts by weight of a propylene-based polymer wax [density: 0.900 g / cm 3 , weight average molecular weight: 7800, softening point 148 ° C., ethylene content: 1.7% by mass], propylene homopolymer [MFR: 1500 g 10 parts, weight average molecular weight: 54000] 20 parts by mass were mixed to obtain a propylene-based polymer composition (6).
Claims (12)
- ゲルパーミエーションクロマトグラフィーにおける排出曲線において、分子量2万以上の位置に少なくとも1つのピークトップと、分子量2万未満の位置に少なくとも1つのピークトップとを有し、極限粘度[η]が0.50(dl/g)~0.75(dl/g)であるプロピレン系重合体からなるメルトブローン不織布。 In the discharge curve in gel permeation chromatography, it has at least one peak top at a molecular weight of 20,000 or more, and at least one peak top at a position of molecular weight less than 20,000, and has an intrinsic viscosity [η] of 0.50. A meltblown non-woven fabric comprising a propylene-based polymer of (dl / g) to 0.75 (dl / g).
- 前記プロピレン系重合体は、重量平均分子量が2万以上である高分子量プロピレン系重合体Aと、重量平均分子量が2万未満である低分子量プロピレン系重合体Bとを少なくとも含む請求項1に記載のメルトブローン不織布。 The propylene-based polymer according to claim 1, wherein the propylene-based polymer comprises at least a high molecular weight propylene polymer A having a weight average molecular weight of at least 20,000 and a low molecular weight propylene polymer B having a weight average molecular weight of less than 20,000. Meltblown non-woven fabric.
- 前記プロピレン系重合体の全質量に対する前記低分子量プロピレン系重合体Bの含有率が、8質量%~40質量%である請求項2に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to claim 2, wherein the content of the low molecular weight propylene polymer B with respect to the total mass of the propylene polymer is 8% by mass to 40% by mass.
- 前記プロピレン系重合体の全質量に対する前記高分子量プロピレン系重合体Aの含有率が、60質量%~92質量%である請求項2又は請求項3に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to claim 2 or 3, wherein the content of the high molecular weight propylene polymer A with respect to the total mass of the propylene polymer is 60% by mass to 92% by mass.
- 前記高分子量プロピレン系重合体Aのメルトフローレート(MFR)が、1000g/10分~2500g/10分である請求項2~請求項4のいずれか1項に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to any one of claims 2 to 4, wherein the melt flow rate (MFR) of the high molecular weight propylene polymer A is 1000 g / 10 minutes to 2500 g / 10 minutes.
- 前記プロピレン系重合体の重量平均分子量は、2万以上である請求項1~請求項5のいずれか1項に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to any one of claims 1 to 5, wherein the weight average molecular weight of the propylene-based polymer is 20,000 or more.
- 平均繊維径が1.1μm未満の繊維で構成される請求項1~請求項6のいずれか1項に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to any one of claims 1 to 6, which is composed of fibers having an average fiber diameter of less than 1.1 μm.
- 比表面積が2.0m2/g~20.0m2/gである請求項1~請求項7のいずれか1項に記載のメルトブローン不織布。 Meltblown nonwoven fabric according to any one of claims 1 to 7 having a specific surface area of 2.0m 2 /g~20.0m 2 / g.
- 平均繊維径に対するピーク繊維径の比率が0.5を超える請求項1~請求項8のいずれか1項に記載のメルトブローン不織布。 The meltblown nonwoven fabric according to any one of claims 1 to 8, wherein the ratio of the peak fiber diameter to the average fiber diameter is more than 0.5.
- 請求項1~請求項9のいずれか1項に記載のメルトブローン不織布を少なくとも含む不織布積層体。 A nonwoven fabric laminate comprising at least the meltblown nonwoven fabric according to any one of claims 1 to 9.
- 請求項1~請求項9のいずれか1項に記載のメルトブローン不織布を含むフィルタ。 A filter comprising the meltblown non-woven fabric according to any one of claims 1 to 9.
- 液体用フィルタである請求項11に記載のフィルタ。 The filter according to claim 11, which is a liquid filter.
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201880062501.9A CN111148872A (en) | 2017-09-26 | 2018-09-26 | Melt-blown nonwoven fabric and filter |
EP18862354.0A EP3674463A4 (en) | 2017-09-26 | 2018-09-26 | Melt-blown nonwoven fabric and filter |
KR1020207010453A KR20200047703A (en) | 2017-09-26 | 2018-09-26 | Meltbloon non-woven fabric and filter |
US16/650,570 US20200222840A1 (en) | 2017-09-26 | 2018-09-26 | Melt-blown nonwoven fabric and filter |
JP2019511799A JP6511595B1 (en) | 2017-09-26 | 2018-09-26 | Meltblown non-woven fabric and filter |
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US (1) | US20200222840A1 (en) |
EP (1) | EP3674463A4 (en) |
JP (1) | JP6511595B1 (en) |
KR (1) | KR20200047703A (en) |
CN (1) | CN111148872A (en) |
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CN112221250B (en) * | 2020-09-10 | 2022-03-22 | 青岛中亚环保工程有限公司 | PBS/PP double-component melt-blown fiber filtering material and manufacturing method thereof |
KR20230121290A (en) | 2022-02-11 | 2023-08-18 | 한화첨단소재 주식회사 | Composite material containing biodegradable polymer, manufacturing method thereof, and melt blown nonwoven fabric containing the composite material |
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- 2018-09-26 EP EP18862354.0A patent/EP3674463A4/en not_active Withdrawn
- 2018-09-26 CN CN201880062501.9A patent/CN111148872A/en active Pending
- 2018-09-26 TW TW107133864A patent/TW201920795A/en unknown
- 2018-09-26 JP JP2019511799A patent/JP6511595B1/en active Active
- 2018-09-26 US US16/650,570 patent/US20200222840A1/en not_active Abandoned
- 2018-09-26 KR KR1020207010453A patent/KR20200047703A/en active IP Right Grant
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Also Published As
Publication number | Publication date |
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JP6511595B1 (en) | 2019-05-15 |
CN111148872A (en) | 2020-05-12 |
KR20200047703A (en) | 2020-05-07 |
TW201920795A (en) | 2019-06-01 |
EP3674463A1 (en) | 2020-07-01 |
EP3674463A4 (en) | 2021-06-16 |
JPWO2019065760A1 (en) | 2019-11-14 |
US20200222840A1 (en) | 2020-07-16 |
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